CN113121744A - Rapid crosslinking and curing water-based polyacrylate and preparation method thereof - Google Patents
Rapid crosslinking and curing water-based polyacrylate and preparation method thereof Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/02—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of acids, salts or anhydrides
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a single or double bond to nitrogen
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- C08F271/00—Macromolecular compounds obtained by polymerising monomers on to polymers of nitrogen-containing monomers as defined in group C08F26/00
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/003—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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Abstract
The invention belongs to the technical field of synthesis of film-forming resin special for paint, and particularly relates to a fast crosslinking and curing water-based polyacrylate and a preparation method thereof, wherein the preparation method comprises the following steps of: and secondly, adding a cationic monomer with a C-C double bond and an acrylic monomer into deionized water in sequence, dropwise adding an initiator solution into the reaction system under the protection of nitrogen to perform prepolymerization reaction, keeping the temperature for 15-45 minutes after the reaction is finished, adding an acrylate monomer, heating to 70-85 ℃, dropwise adding the initiator solution into the reaction system under the protection of nitrogen to perform polymerization reaction, keeping the temperature for 80-100 minutes, and adjusting the pH value of the system to 7.5-8.5 by using an alkaline solution after the reaction is finished to obtain the water-based polyacrylate emulsion. The invention realizes the rapid curing of the water-based polyacrylate emulsion and improves the stability of the acrylic resin emulsion.
Description
Technical Field
The invention belongs to the technical field of synthesis of film-forming resin special for paint, and relates to rapidly cross-linked and cured water-based polyacrylate and a preparation method thereof.
Background
The acrylic resin coating has the advantages of good chemical corrosion resistance, oil resistance, weather resistance, stain resistance, transparency, construction performance and the like, and is widely applied to the fields of plastic products, metal products, coil industry, textiles, wood products, building, paper making industry and the like. The solvent type acrylic resin coating can release a large amount of Volatile Organic Compounds (VOC) in the construction and drying processes, and causes great harm to human bodies and the environment. In recent years, the waterborne acrylic resin coating has the advantages of convenience in construction, environmental friendliness and the like, and becomes an industry development trend. The acrylic resin emulsion is one of waterborne acrylic resins, and has wide market application.
For example, in chinese patent nos. CN201010528305.1 and CN202011293347.1, ionic emulsifiers (such as polyoxyethylene ether sulfonate, phosphate surfactants, etc.) or nonionic emulsifiers (such as polyoxyethylene alkyl ethers, etc.) are usually added during the synthesis of acrylic resin emulsion, and these additional surfactants cannot be chemically bonded with acrylate molecular chains, which greatly affects the dispersion stability of acrylic resin emulsion and the water resistance and color of coating. To this end, this problem is solved by copolymerization of reactive anionic emulsifiers (e.g.allylpolyoxyethylene ether sulphate) with acrylate monomers. However, the polyacrylate molecular chain has longer chain segment of the reactive anionic emulsifier, so that the crosslinking curing time of the acrylic resin coating is prolonged.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of a rapid crosslinking and curing water-based polyacrylate.
Another object of the present invention is to provide a rapidly crosslinking-curing aqueous polyacrylate.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of fast crosslinking cured water-based polyacrylate comprises the following steps,
step one, preparing acrylic acid prepolymer dispersion liquid: sequentially adding a cationic monomer with C-C double bond and an acrylic acid monomer into deionized water, dropwise adding 10-25 wt% of initiator solution into a reaction system while stirring under the protection of nitrogen for prepolymerization reaction, and after dropwise adding, keeping the temperature for reaction for 15-45 minutes to obtain an acrylic acid prepolymer dispersion liquid,
and step two, adding an acrylate monomer into the acrylic acid prepolymer dispersion liquid obtained in the step one, carrying out ultrasonic oscillation for 20-50 minutes, heating to 70-85 ℃, stirring while dropwise adding 10-25 wt% of initiator solution into the reaction system under the protection of nitrogen to initiate polymerization reaction, carrying out heat preservation reaction for 80-100 minutes after dropwise adding, and adjusting the pH value of the system to 7.5-8.5 by using an alkaline solution after the reaction is finished, thus obtaining the water-based polyacrylate emulsion.
In the preparation method of the fast crosslinking cured water-based polyacrylate, in the step one, the molar ratio of the cationic monomer to the acrylic acid monomer is 0.5-2:1, and the total mass of the cationic monomer and the acrylic acid monomer is as follows: the mass of the deionized water is 0.15-0.30:1, and the total mass of the cationic monomer and the acrylic acid monomer is as follows: the mass of the initiator solution is 1:0.01-0.02,
in the preparation method of the fast crosslinking cured water-based polyacrylate, in the second step, the molar ratio of the acrylate monomer to the acrylic monomer is 1-2: 1;
a preparation method of fast crosslinking cured water-based polyacrylate comprises the following steps,
step one, preparing acrylic acid prepolymer dispersion liquid: sequentially adding a cationic monomer with a C ═ C double bond and an acrylic acid monomer into deionized water according to a molar ratio of 0.5-2:1, wherein the total mass of the cationic monomer and the acrylic acid monomer is as follows: the mass of the deionized water is 0.15-0.30:1, 10-25 wt% of initiator solution is dripped into the reaction system while stirring under the protection of nitrogen for prepolymerization reaction, and the total mass of the cationic monomer and the acrylic monomer is as follows: the mass of the initiator solution is 1:0.01-0.02, and the acrylic acid prepolymer dispersion liquid is prepared after the dropping reaction is carried out for 15-45 minutes by heat preservation;
adding an acrylate monomer into the acrylic prepolymer dispersion liquid obtained in the step one, wherein the molar ratio of the acrylate monomer to the acrylic monomer is 1-2: 1; after ultrasonic oscillation for 20-50 minutes, heating to 70-85 ℃, stirring while dropping 10-25 wt% of initiator solution into the reaction system under the protection of nitrogen to initiate polymerization reaction, keeping the temperature for 80-100 minutes after dropping, and adjusting the pH value of the system to 7.5-8.5 by using alkaline solution after the reaction is finished to obtain the water-based polyacrylate emulsion.
In the above method for preparing a fast crosslinking cured waterborne polyacrylate, the cationic monomer having a C ═ C double bond is one of allyl trimethyl ammonium chloride, allyl trimethyl ammonium bromide, diallyl dimethyl ammonium chloride, diallyl methyl propyl ammonium bromide, diallyl methyl pentyl ammonium bromide, diallyl methyl heptyl ammonium bromide or diallyl methyl nonyl ammonium bromide.
In the preparation method of the rapidly cross-linked and cured waterborne polyacrylate, the acrylate monomer is one or more of methyl methacrylate, ethyl methacrylate, isopropyl methacrylate, n-butyl methacrylate, isobutyl methacrylate, hexyl methacrylate, cyclohexyl methacrylate, isobornyl methacrylate, n-butyl acrylate, isobutyl acrylate, ethyl acrylate, n-octyl acrylate, isooctyl acrylate or isobornyl acrylate.
In the preparation method of the fast crosslinking cured water-based polyacrylate, the initiator solution is one of azodiisobutyl amidine hydrochloride aqueous solution or ammonium persulfate aqueous solution.
In the preparation method of the fast crosslinking cured water-based polyacrylate, the alkaline solution is one of a sodium carbonate solution, a sodium acetate solution, sodium dihydrogen phosphate or disodium hydrogen phosphate solution with the mass percentage concentration of 10-20%.
In the preparation method of the fast crosslinking cured water-based polyacrylate, the acrylic acid monomer is one or more of acrylic acid or methacrylic acid.
A fast crosslinking cured waterborne polyacrylate.
Compared with the prior art, the invention has the advantages that:
the invention adopts a special cationic monomer with C ═ C double bond, and the copolymerization of (methyl) acrylic acid and acrylate monomer to prepare the water-based polyacrylate emulsion, which has the advantages that: (1) after the cationic monomer with C ═ C double bonds, the (methyl) acrylic acid and the (methyl) acrylate monomer are copolymerized, the molecular chain of the prepared polyacrylate has ammonium ions with positive charges and carboxylate ions with negative charges, and when the coating is cured, strong adsorption crosslinking action can be generated among the molecular chains, so that the curing time of the coating is shortened, and quick curing can be realized; (2) the cationic monomer with C ═ C double bonds is a special cationic surfactant, can play an emulsifying function, does not need to be additionally added with other emulsifying agents, and improves the stability of the aqueous acrylic resin emulsion.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the present invention will be clearly and completely described below with reference to the specific embodiments.
Example 1
A preparation method of fast crosslinking cured water-based polyacrylate comprises the following steps,
1. sequentially adding 6.75 kg of allyl trimethyl ammonium chloride and 8.6 kg of methacrylic acid into 102 kg of deionized water, dropwise adding 1.54 kg of azodiisobutyl amidine hydrochloride solution with the mass percentage concentration of 10% into a reaction system while stirring under the protection of nitrogen to perform prepolymerization reaction, and after dropwise adding, performing heat preservation reaction for 15 minutes to obtain an acrylic prepolymer dispersion liquid;
2. and (2) adding 10 kg of methyl methacrylate into the acrylic acid prepolymer dispersion liquid obtained in the step (1), oscillating for 20 minutes by ultrasonic waves, heating to 70 ℃ under the protection of nitrogen, dropwise adding 10% by mass of ammonium persulfate solution into the reaction system while stirring to initiate polymerization, keeping the temperature for 80 minutes after dropwise adding, and adjusting the pH value of the system to 7.5 by using 10% by mass of sodium carbonate solution after the reaction is finished to obtain the water-based polyacrylate emulsion.
Example 2
A preparation method of fast crosslinking cured water-based polyacrylate comprises the following steps,
1. adding 18 kg of allyl trimethyl ammonium bromide and 8.6 kg of methacrylic acid into 88.7 kg of deionized water in sequence, dropwise adding 2.13 kg of ammonium persulfate solution with the mass percentage concentration of 25% into a reaction system while stirring under the protection of nitrogen to perform prepolymerization reaction, and after dropwise adding, keeping the temperature for reaction for 45 minutes to obtain the acrylic acid prepolymer dispersion liquid.
2. Adding 22.8 kg of ethyl methacrylate into the acrylic acid prepolymer dispersion liquid obtained in the step 1, carrying out ultrasonic oscillation for 35 minutes, heating to 85 ℃ under the protection of nitrogen, dropwise adding azodiisobutyl amidine hydrochloride solution with the mass percentage concentration of 25% into the reaction system while stirring to initiate polymerization, carrying out heat preservation reaction for 100 minutes after dropwise adding, and adjusting the pH value of the system to 8.5 by using sodium carbonate solution with the mass percentage concentration of 20% after the reaction is finished, thus obtaining the water-based polyacrylate emulsion.
Example 3
A preparation method of fast crosslinking cured water-based polyacrylate comprises the following steps,
1. adding 19.2 kg of diallyl dimethyl ammonium chloride and 8.6 kg of acrylic acid into 139 kg of deionized water in sequence, dropwise adding 2.78 kg of azodiisobutyl amidine hydrochloride solution with the mass percentage concentration of 15% into the reaction system while stirring under the protection of nitrogen to perform prepolymerization reaction, and after dropwise adding, keeping the temperature for reaction for 30 minutes to obtain the acrylic acid prepolymer dispersion liquid.
2. Adding 22.9 kg of isopropyl methacrylate into the acrylic acid prepolymer dispersion liquid obtained in the step 1, carrying out ultrasonic oscillation for 35 minutes, heating to 80 ℃ under the protection of nitrogen, dropwise adding an ammonium persulfate solution with the mass percentage concentration of 15% into the reaction system while stirring to initiate polymerization reaction, carrying out heat preservation reaction for 90 minutes after dropwise adding, and adjusting the pH value of the system to be 8 by using a sodium carbonate solution with the mass percentage concentration of 15% after the reaction is finished, thus obtaining the water-based polyacrylate emulsion.
Example 4
A preparation method of fast crosslinking cured water-based polyacrylate comprises the following steps,
1. 21.9kg of diallyl methyl propyl ammonium bromide and 8.6 kg of acrylic acid are sequentially added into 122 kg of deionized water, 3.05 kg of azobisisobutylamidine hydrochloride solution with the mass percentage concentration of 20% is dropwise added into the reaction system while stirring under the protection of nitrogen for prepolymerization reaction, and after the dropwise addition, the thermal insulation reaction is carried out for 25 minutes, thus obtaining the acrylic acid prepolymer dispersion liquid.
2. Adding 16.9 kg of n-butyl methacrylate into the acrylic acid prepolymer dispersion liquid obtained in the step 1, oscillating for 40 minutes by ultrasonic waves, heating to 75 ℃ under the protection of nitrogen, dropwise adding an ammonium persulfate solution with the mass percentage concentration of 25% into a reaction system while stirring to initiate polymerization reaction, keeping the temperature for reaction for 85 minutes after dropwise adding, and adjusting the pH value of the system to 8.5 by using a sodium carbonate solution with the mass percentage concentration of 10% after the reaction is finished to obtain the water-based polyacrylate emulsion.
Comparative example 1
In comparative example 1, the diallylmethylpropylammonium bromide procedure of example 4 was removed, and the other process conditions were unchanged, with the following specific operating steps:
1. adding 8.6 kg of acrylic acid into 122 kg of deionized water, dropwise adding 3.05 kg of azobisisobutylamidine hydrochloride solution with the mass percentage concentration of 20% into the reaction system while stirring under the protection of nitrogen for prepolymerization, and after dropwise adding, carrying out heat preservation reaction for 25 minutes to obtain the acrylic acid prepolymer dispersion liquid.
2. Adding 16.9 kg of n-butyl methacrylate into the acrylic acid prepolymer dispersion liquid obtained in the step 1, oscillating for 40 minutes by ultrasonic waves, heating to 75 ℃ under the protection of nitrogen, dropwise adding an ammonium persulfate solution with the mass percentage concentration of 25% into a reaction system while stirring to initiate polymerization reaction, keeping the temperature for reaction for 90 minutes after dropwise adding, and adjusting the pH value of the system to 8.5 by using a sodium carbonate solution with the mass percentage concentration of 10% after the reaction is finished to obtain the water-based polyacrylate emulsion.
Comparative example 2
In comparative example 1, the acrylic acid step in example 4 was removed, and other process conditions were unchanged, and the specific operation steps were as follows:
1. adding 21.9kg of diallyl methyl propyl ammonium bromide into 122 kg of deionized water, dropwise adding 3.05 kg of azodiisobutyl amidine hydrochloride solution with the mass percentage concentration of 20% into the reaction system while stirring under the protection of nitrogen to perform prepolymerization reaction, and after dropwise adding, keeping the temperature and reacting for 25 minutes to obtain the cationic prepolymer dispersion liquid containing C-C double bonds.
2. Adding 16.9 kg of n-butyl methacrylate into the cationic prepolymer dispersion liquid containing C ═ C double bonds obtained in the step 1, oscillating for 40 minutes by ultrasonic waves, heating to 75 ℃ under the protection of nitrogen, dropwise adding 25% by mass of ammonium persulfate solution into the reaction system while stirring to initiate polymerization reaction, keeping the temperature for reaction for 85 minutes after dropwise adding, and adjusting the pH value of the system to 8.5 by 10% by mass of sodium carbonate solution after the reaction is finished, thus obtaining the water-based polyacrylate emulsion.
Evaluation of coating Properties
The emulsions prepared in the examples and comparative examples were evaluated by performance tests, in which the aqueous polyacrylate emulsion was brush coated on an ABS engineering plastic sheet, the substrate was heated to 80 ℃ and the curing time was measured, and the test results are shown in Table 1. As can be seen from Table 1, the polyacrylate emulsion prepared by the invention has short curing time and good emulsion stability.
TABLE 1 evaluation of the Properties of emulsions obtained in examples of the invention and comparative examples
| Performance of | Curing time/min | Storage stability of emulsions |
| Example 1 | 6 | No delamination in 1 year |
| Example 2 | 6 | No delamination in 1 year |
| Example 3 | 6 | No delamination in 1 year |
| Example 4 | 5 | No delamination in 1 year |
| For comparison 1 | 13 | Half year stratification |
| For comparison 2 | 12 | Half year stratification |
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit of the invention.
Claims (10)
1. A preparation method of fast crosslinking cured water-based polyacrylate is characterized by comprising the following steps,
step one, preparing acrylic acid prepolymer dispersion liquid: sequentially adding a cationic monomer with C-C double bond and an acrylic acid monomer into deionized water, dropwise adding 10-25 wt% of initiator solution into a reaction system while stirring under the protection of nitrogen for prepolymerization reaction, and after dropwise adding, keeping the temperature for reaction for 15-45 minutes to obtain an acrylic acid prepolymer dispersion liquid,
and step two, adding an acrylate monomer into the acrylic acid prepolymer dispersion liquid obtained in the step one, carrying out ultrasonic oscillation for 20-50 minutes, heating to 70-85 ℃, stirring while dropwise adding 10-25 wt% of initiator solution into the reaction system under the protection of nitrogen to initiate polymerization reaction, carrying out heat preservation reaction for 80-100 minutes after dropwise adding, and adjusting the pH value of the system to 7.5-8.5 by using an alkaline solution after the reaction is finished, thus obtaining the water-based polyacrylate emulsion.
2. The method for preparing the rapidly cross-linking and curing water-based polyacrylate according to claim 1, wherein in the first step, the molar ratio of the cationic monomer to the acrylic monomer is 0.5-2:1, and the total mass of the cationic monomer to the acrylic monomer is as follows: the mass of the deionized water is 0.15-0.30:1, and the total mass of the cationic monomer and the acrylic acid monomer is as follows: the mass of the initiator solution is 1: 0.01-0.02.
3. The method for preparing the rapidly cross-linking and curing water-based polyacrylate according to claim 1, wherein in the second step, the molar ratio of the acrylate monomer to the acrylic acid monomer is 1-2: 1.
4. A preparation method of fast crosslinking cured water-based polyacrylate is characterized by comprising the following steps,
step one, preparing acrylic acid prepolymer dispersion liquid: sequentially adding a cationic monomer with a C ═ C double bond and an acrylic acid monomer into deionized water according to a molar ratio of 0.5-2:1, wherein the total mass of the cationic monomer and the acrylic acid monomer is as follows: the mass of the deionized water is 0.15-0.30:1, 10-25 wt% of initiator solution is dripped into the reaction system while stirring under the protection of nitrogen for prepolymerization reaction, and the total mass of the cationic monomer and the acrylic monomer is as follows: the mass of the initiator solution is 1:0.01-0.02, and the acrylic acid prepolymer dispersion liquid is prepared after the dropping reaction is carried out for 15-45 minutes by heat preservation;
adding an acrylate monomer into the acrylic prepolymer dispersion liquid obtained in the step one, wherein the molar ratio of the acrylate monomer to the acrylic monomer is 1-2: 1; after ultrasonic oscillation for 20-50 minutes, heating to 70-85 ℃, stirring while dropping 10-25 wt% of initiator solution into the reaction system under the protection of nitrogen to initiate polymerization reaction, keeping the temperature for 80-100 minutes after dropping, and adjusting the pH value of the system to 7.5-8.5 by using alkaline solution after the reaction is finished to obtain the water-based polyacrylate emulsion.
5. The method of claim 1 or 4, wherein the cationic monomer having a C ═ C double bond is one of allyl trimethyl ammonium chloride, allyl trimethyl ammonium bromide, diallyl dimethyl ammonium chloride, diallyl methyl propyl ammonium bromide, diallyl methyl pentyl ammonium bromide, diallyl methyl heptyl ammonium bromide or diallyl methyl nonyl ammonium bromide.
6. The method for preparing the rapidly cross-linking and curing water-based polyacrylate according to claim 1 or 4, wherein the acrylate monomer is one or more of methyl methacrylate, ethyl methacrylate, isopropyl methacrylate, n-butyl methacrylate, isobutyl methacrylate, hexyl methacrylate, cyclohexyl methacrylate, isobornyl methacrylate, n-butyl acrylate, isobutyl acrylate, ethyl acrylate, n-octyl acrylate, isooctyl acrylate or isobornyl acrylate.
7. The method of claim 1 or 4, wherein the initiator solution is one of aqueous azobisisobutylamidine hydrochloride or aqueous ammonium persulfate.
8. The method for preparing a rapidly cross-linking curable aqueous polyacrylate according to claim 1 or 4, wherein the alkaline solution is one of a sodium carbonate solution, a sodium acetate solution, a sodium dihydrogen phosphate solution or a disodium hydrogen phosphate solution at a concentration of 10-20% by mass.
9. The method for preparing the rapidly cross-linking cured waterborne polyacrylate of claim 1 or 4, wherein the acrylic acid monomer is one or more of acrylic acid or methacrylic acid.
10. A fast crosslinking cured aqueous polyacrylate obtained by the method of preparing a fast crosslinking cured aqueous polyacrylate according to any one of claims 1 to 9.
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